In accordance with the present invention, this end has been attained by a novel processing sequence wherein a weak acetate ligand in combination with a hydroxide solution with a balanced pH permits the formation of fine particles of a mixed hydroxide-acetate composition. More specifically, there is described herein a method for the synthesis of LiMn.sub.2 O.sub.4 and LiCoO.sub.2 phases by a novel sol-gel process involving the condensation of oxide networks from solution precursors. Briefly, this involves hydrolyzing manganese or cobalt acetates or other carboxylates in an aqueous solution, the hydrolysis being promoted by the addition of the hydroxides of lithium and ammonium which control the pH of the solution. Hydrolysis is initiated by the addition of lithium hydroxide and completed by the use of a base that can be removed thermally. This base may be selected from among any organic base or ammonium hydroxide which is preferred for use herein. This low temperature process yields a gel-like product which may be used to prepare either bulk or thick films of LiMn.sub.2 O.sub.4 or LiCoO.sub.2 which evidence electrochemical properties suitable for use in rocking chain batteries.